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Micro-channel chemical preparation method of porous metal-organic framework material

An organic framework and porous metal technology, applied in the field of microchannel chemical preparation of porous metal organic framework materials, can solve the problems of large equipment volume, long residence time, poor mixing effect, etc., and achieve the effect of high surface area

Inactive Publication Date: 2015-09-09
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

They have a large processing capacity and can meet the requirements of large-scale industrial production, but they also have the disadvantages of poor mixing effect, large equipment volume and long residence time.

Method used

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  • Micro-channel chemical preparation method of porous metal-organic framework material
  • Micro-channel chemical preparation method of porous metal-organic framework material
  • Micro-channel chemical preparation method of porous metal-organic framework material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Add 12g of copper acetate to 350ml of deionized water to make solution A, add 8g of trimesic acid to 350ml of ethanol to make solution B; filter A and B, add T-type quartz at a flow rate of 0.5ml / min In the two inlet microchannels of the circular hole microchannel reactor, the angle between the inlet microchannels is 180°, and the angle between each inlet microchannel and the reaction microchannel is 90°, the length of the reaction microchannel is 8m, and the inner diameter is 0.23mm , the microchannel reaction temperature is 80°C; react for 8 hours, and collect the product directly. After filtering, washing once with 200ml of ethanol and once with 100ml of acetone, and drying at 60°C for 6 hours, 9g of porous Cu-BTC framework material was obtained.

[0048] N 2 The specific surface area is 876m 2 / g (as determined by the Langmuir method).

[0049] figure 1 It is the particle size distribution diagram of the obtained product (measured by Malvern particle size analyz...

Embodiment 2

[0051] Add 12g of copper acetate to 250ml of deionized water to make solution A, add 8g of trimesic acid to 250ml of ethanol to make solution B; filter A and B, add T-type quartz at a flow rate of 0.5ml / min In the two inlet microchannels of the circular hole microchannel reactor, the angle between the inlet microchannels is 180°, and the angle between each inlet microchannel and the reaction microchannel is 90°, the length of the reaction microchannel is 8m, and the inner diameter is 0.23mm , the microchannel reaction temperature is 80°C; collect the feed liquid at the outlet of the reactor, then transfer the feed liquid into the reactor, and age at 100°C for 10h. After filtering, washing once with 200ml of ethanol and once with 100ml of acetone, and drying at 60°C for 6 hours, 12g of porous Cu-BTC framework material was obtained.

[0052] N 2 The specific surface area is 1013m 2 / g (as determined by the Langmuir method).

[0053] figure 2 It is the particle size distribu...

Embodiment 3

[0055] Add 36g of copper acetate to 1050ml of deionized water to make solution A, add 25g of trimesic acid to 1050ml of ethanol to make solution B; filter A and B, add T-shaped quartz circle at a flow rate of 3ml / min In the two inlet microchannels of the well microchannel reactor, the angle between the inlet microchannels is 90°, the angle between the B liquid inlet microchannel and the reaction microchannel is 90°, the length of the reaction microchannel is 10m, and the inner diameter is 0.5mm. The channel reaction temperature is 80°C; react for 3 hours, collect the product directly, and then enter the feed liquid into a 2L reactor for aging reaction at 100°C for 10 hours. After filtering, washing once with 200ml of ethanol and once with 100ml of acetone, and drying at 80°C for 4 hours, 15g of porous Cu-BTC framework material was obtained.

[0056] N 2 The specific surface area is 1076m 2 / g (as determined by the Langmuir method).

[0057] image 3 It is the particle size...

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Abstract

The purpose of the invention is providing a micro-channel chemical preparation method of porous metal-organic framework material. The method comprises the following steps: respectively injecting a liquid medium containing one or more organic compounds with at least one unidentate ligand, a liquid medium containing one or more metal ions, a liquid medium containing a deprotonation assistant and an inert gas into a micro-channel reactor through different inlets, carrying out a coordination reaction on the above obtained mixed material liquid in the micro-channel at a certain temperature under a certain pressure to form a coordination compound, crystallizing, filtering, washing, and drying to prepare the porous metal-organic framework material, wherein the micro-channel reactor has at least two inlets and one outlet; the addition amount of the deprotonation assistant is 0-50% of the mole number of all metal ions; a ratio of the volume velocity of inert gas added into the micro-channel reactor to the bulk volume velocity of the liquid phase is 0-100:1; and the crystallization process can be omitted. The method has the characteristics of simple and safe operation, high efficiency, large throughput and easy amplification.

Description

technical field [0001] The invention belongs to the field of new materials and synthetic chemistry, and in particular relates to a microchannel chemical preparation method of a porous metal organic framework material. Background technique [0002] Metal-Organic Frameworks (MOFs) materials are a new type of porous materials that have developed most rapidly in the past decade. This supramolecular network structure formed by the self-assembly of organic ligands and metal ions has a specific pore distribution and a large specific surface area similar to inorganic molecular sieve materials. Compared with traditional porous materials such as zeolite and activated carbon, this type of material has the characteristics of large adsorption capacity, highly ordered pore structure, low crystal density, high specific area, and adjustable pore shape and size. Ligands can regulate the properties of the pore surface, etc., and can achieve the purpose of increasing the adsorption affinity f...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C63/307C07C51/00C07D233/58C07C57/15
CPCC07F1/005C07C51/418C07C57/15C07C63/307C07D233/58C07F3/003C07F5/003
Inventor 王树东孙天军胡江亮任新宇
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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